反应详情

Methanesulfonic acid 4-methyl-3-nitro-benzyl ester (0.45 g, 1.83 mmol) was added to anhydrous DMF (20 mL), under argon, and potassium phthalimide (0.34 g, 1.83 mmol) was added. The reaction mixture was heated to 60EC for 12 h. The reaction mixture was cooled and poured into 1N HCl and the aqueous layer was extracted three times with ethyl acetate. The combined organic layers were washed with water, brine and dried over anhydrous magnesium sulfate. The solution was filtered and the solvent removed under reduced pressure. The product was isolated by flash chromatography. (4:1 hexane/ethyl acetate) Yield 0.45 g. 1H NMR (CDCl3, 300 MHz): δ 2.58 (s, 3H), 4.88 (s, 2H), 7.30 (d, J=7 Hz, 1H), 7.57 (d, J=7 Hz, 1H), 7.24-7.77 (m, 2H), 7.84-7.89 (m, 2H), 8.02 (s, 1H).

1. temperatureThe reaction mixture was heated to 60EC for 12 h
2. temperatureThe reaction mixture was cooled
3. extractionthe aqueous layer was extracted three times with ethyl acetate
4. washThe combined organic layers were washed with water, brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe solution was filtered
7. customthe solvent removed under reduced pressure
8. customThe product was isolated by flash chromatography